153 resultados para Validação de Metodologia Analítica
Resumo:
A rapid and efficient analytical method is presented for the quantitative analysis of 10 organochlorine pesticides in corn meal. The extraction and clean up steps are combined into one step by transferring the sample to a chromatographic column prepacked with alumina and silica gel. The pesticides are eluted with n-hexane-dichloromethane 9:1 (v/v) and the extracts analized by gas-liquid chromatography with electron capture detection, the average recoveries were between 78% and 98% and the detection limits were between 1 and 5 ng/g.
Resumo:
The efficiency of two methods for determining 3-hydroxybutyrate and 3-hydroxyvalerate content in the biopolymer (poly(3-hydroxybutyrate-co-3-hydroxyvalerate) has been evaluated. Both methods are based on (a) the hydrolysis of polymers, (b) the esterification with methyl (method A) and isoamilic alcohol (method B) and (c) analysis of the esters by gas chromatography using flame ionization detection (GC-FID). After optimization of the analytical conditions, the main validation parameters (linearity, quantification limit, detection limit, recovery, sensitivity and precision) were determined showing that both analytical procedures can be applied to control the process of poly(3-hydroxybutyrate) production. However, method B gives better analytical results than method A and has the advantage of not using chlorinated solvents.
Resumo:
The present article deals with the adaptation of the Moral Judgment Test (MJT) for the Portuguese language. The principles of the test, its format and the process of content, construct and criterion validation are presented. In the same way, reliability is discussed using Brazilian research results that produced the necessity of elaborating another dilemma to compose the MJT-xt (extended).
Resumo:
The response surface methodology as a tool for assessing the production of alginate and polyhydroxybutirate by Azotobacter vinelandii. Alginate is a polysaccharide extracted from cell walls of brown algae and used in the food, pharmaceuticals and biotech industries. Production is concentrated on the cultivation of brown seaweed, but several bacteria of the genus Pseudomonas and Azotobacter produce alginate. The chemical structure of alginates produced by algae is similar to those synthesized by A. vinelandii. The bacteria also produce intracellular polymers such as polyhydroxybutyrate (PHB), known as bioplastic. This work studied the simultaneous alginate and PHB production by A. vinelandii using sucrose and different parameters of fermentation in an orbital shaker. The optimal values for the production of these compounds were determined by the MSR. The first experiment was a 2(6-2) factorial design. The second was based on significant variables of the first, resulting in a full 3(3-0) factorial design. From the first to the second, an increase was observed in the PHB productivity from 12 to 45 mg g(-1) cell h(-1) and alginate from 100 to 1,600 mg g(-1) of cell h(-1). The productivity of both compounds was in the maximum incubation temperature of 62 degrees C, in the shortest time of incubation (18h) and the sucrose concentration, 11 g L(-1). In both experiments the PHB extracted presented purity of 94%.
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A coal deposit was studied at Sapopema (PR) in the upper part of the Tubarao Group. The eliptical deposit is made up by a single layer of 1.2 m mean thickness and lies at a depth of 380 to 700 m. The semi-variogram, using the spherical model, revealed a range of 1.5 km and no nugget effect. Area kriging estimation for a grid of 0.5 × 0.5 km showed a value of 50.121.750 ton, very close to the real reserve one. -from English summary
Resumo:
This work develops a methodology (using the degree-days concept and linear regression), to forecast the duration of phenological phases in crops. An experiment was conducted in the greenhouse with three cultivars of cowpea (Vigna unguiculata (L.) Walp.), cv. Califórnia-781, Tvx 5058-09C and IT 81D-1032. The methodology was based on the relative thermal efficiency rate, determined for each species or cv. The results show that the proposed methodology may be a good alternative in works involving crops, especially because it does not require the repetition of the experiments.
Resumo:
This work presents an algorithm for the security control of electric power systems using control actions like generation reallocation, determined by sensitivity analysis (linearized model) and optimization by neural networks. The model is developed taking into account the dynamic network aspects. The preventive control methodology is developed by means of sensitivity analysis of the security margin related with the mechanical power of the system synchronous machines. The reallocation power in each machine is determined using neural networks. The neural network used in this work is of Hopfield type. These networks are dedicated electric circuits which simulate the constraint set and the objective function of an optimization problem. The advantage of using these networks is the higher speed in getting the solutions when compared to conventional optimization algorithms due to the great convergence rate of the process and the facility of the method parallelization. Then, the objectives are: formulate and investigate these networks implementations in determining. The generation reallocation in digital computers. Aiming to illustrate the proposed methodology an application considering a multi-machine system is presented.
Resumo:
Chemically modified electrodes based on hexacyanometalate films are presented as a tool in analytical chemistry. Use of amperometric sensors and/or biosensors based on the metal-hexacyanoferrate films is a tendency. This article reviews some applications of these films for analytical determination of both inorganic (e.g. As3+, S2O3 2-) and organic (e.g. cysteine, hydrazine, ascorbic acid, gluthatione, glucose, etc.) compounds.
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In this work was developed an alternative methodology to separation of aquatic organic matter (AOM) present in natural river waters. The process is based in temperature decreasing of the aqueous sample under controlled conditions that provoke the freezing of the sample and separation of the dark extract, not frozen and rich in organic matter. The results showed that speed of temperature decreasing exerts strongly influence in relative recovery of organic carbon, enrichment and time separation of the organic matter present in water samples. Elemental composition, infrared spectra and thermal analysis results showed that the alternative methodology is less aggressive possible in the attempt of maintaining the integrity of the sample.
Resumo:
Human platelet-derived growth factor (PDGF) was purified from lysates of clinically outdated human platelets by ionic exchange chromatography in CM-Sepharose. The eluated fraction was submitted to the Immunoblot/Slot Blot assay using anti-PDGF-AA and anti-PDGF-BB polyclonal antibodies and was evaluated as to its biological activity through the test of [H 3]-thymidine incorporation in NIH/3T3 cell line fibroblasts in culture. The Immunoblot/Slot Blot assay using anti-PDGF-AA and anti-PDGF-BB antibodies proved the presence of the PDGF in chromatographic cationic fraction. The comparison of biological activities between fiblobrast stimulation assay using recombinant PDGF-AB and partially purified PDGF was demonstrated in 165.796 and 157.567 cpm, respectively. This result, proved the potent mitogenic effect of partially purified PDGF and consequently their evidence about the wound healing activity.
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Haematological investigation is an important part of disease diagnosis. The techniques used for mammals are generally applicable for fishes with slight modification. The presence of nucleated erythrocytes and thrombocytes in fish may cause some confusion in the identification of blood cells, mainly in total leukocytes count. This work evaluated two different methods (direct and indirect) of leukocytes counting. Specimens of tilapia were divided randomly into four groups of 48 fish each. Each group was further randomized into three replicate experiments of 16 fish per replicate in 40 L aquarium and maintained for 10 days. Counting of leukocytes in peripheral blood was determined in six fishes per group at the times: 0, 3, 7 and 10 days. The direct method in Neubauer chamber showed a large dispersion of data in regard to the average, the opposite was observed in indirect method determined in blood smears that showed more homogeneity among groups. Due to this factor the indirect method can be considered more accurate than the direct method for counting leukocytes in fishes.
Resumo:
Soil flushing is an alternative remediation technology for soils contaminated with heavy metals, which the main contaminant removing process consists in percolating an extraction solution. This work aimed to use the response surface methodology to point out combinations among the parameters of the extraction solution (Na2EDTA concentration, volume e pH) in order to reduce the concentration of copper in a sandy soil to risk levels lower than the intervention levels for exposure scenarios adopted by the Environmental Company of Sao Paulo State. Thus, a series of tests in leaching columns were carried out using a Fluvisol artificially contaminated (1257,3 mg kg-1). The tests were conducted in triplicate and setup a central composite rotatable design with 15 different parameters combinations of the extraction solution and one replicate in the center point. Using 5% significance level, the adjusted model (R2 = 0,98) indicated combinations of Na2EDTA concentration, pH and volume of the extraction solution which allow reduction of copper concentration below levels reported by environmental agency of Sao Paulo State for industrial, residential, agricultural or maximum exposure scenarios.
Resumo:
Estudos sobre as mais diversas formas de controle de pragas e utilização de inimigos naturais, exigem artrópodes em quantidade e qualidade. Mediante essa necessidade, o processo de criação e multiplicação de artrópodes, vem ao longo dos anos, passando por significativas transformações. As técnicas de criação e multiplicação de insetos são muito importantes em estudos de biologia e de métodos de controle. A criação e definição de uma metodologia para multiplicação tem sido um grande desafio nos estudos da biologia e da criação de insetos, principalmente, devido a dificuldade de estabelecimento de populações em casa de vegetação e campo. Visando otimizar e adequar uma metodologia de multiplicação de Aphis gossypii (Hemiptera: Aphididae) em condições de laboratório, foi estabelecida uma colônia sobre plantas de algodoeiro (Gossypium hirsutum L. raça Latifolium Hutch) objetivando uma melhoria nas condições de sobrevivência e multiplicação desses insetos, menores influencias dos fatores abióticos, e a potencialização do uso das plantas por um período mais longo. Com o desenvolvimento dessa técnica e dos recursos utilizados na criação, notou-se um incremento na quantidade de indivíduos obtidos, melhor aproveitamento das plantas e diminuição de custos. Dessa forma evitou-se também a migração e infestação de outras espécies de pulgões e a ação de inimigos naturais. Após o estabelecimento da criação, verificou-se que o controle do parasitismo de A. gossypii foi de acordo com as condiçõ es submetida.
Resumo:
Due necessity of better understanding leptin and reproduction relations, a specific radioimmunoassay (RIA) to bovine leptin was avalidated. First, an antibody production protocol was developed using recombinant equine leptin inoculated in a rabbit, that results in 28,05% of maximum binding (MB) 105 days after the protocol beginning. The tests of validations verified parallelism between standard curve and dilutions of high and low controls (P < 0,01). Antibody against equine leptin showed specificity to bovine leptin (P < 0,01). The recuperation tax of bovine leptin by antibody against recombinant equine leptin was from 98,4 to 101,6% (P < 0, 01). When the samples were stored in ambient temperature or refrigerated to 4°C, ligation stability was verified (P > 0,2), however, temperatures above 37°C impaired the bovine leptin recuperation. The use of assay buffer with or without bovine plasma did not show any difference (P > 0,3). These results showed that the antibody produced in rabbit against equine leptin were able to detect plasmatic bovine leptin, and that the RIA to bovine leptin quantification had adequate characteristics to the development of a valid assay.
Resumo:
Triamcinolone (TRI), a drug widely used in the treatment of ocular inflammatory diseases, is practically insoluble in water, which limits its use in eye drops. Cyclodextrins (CDs) have been used to increase the solubility or dissolution rate of drugs. The purpose of the present study was to validate a UV-Vis spectrophotometric method for quantitative analysis of TRI in inclusion complexes with beta-cyclodextrin (B-CD) associated with triethanolamine (TEA) (ternary complex). The proposed analytical method was validated with respect to the parameters established by the Brazilian regulatory National Agency of Sanitary Monitoring (ANVISA). The analytical measurements of absorbance were made at 242nm, at room temperature, in a 1-cm path-length cuvette. The precision and accuracy studies were performed at five concentration levels (4, 8, 12, 18 and 20μg.mL -1). The B-CD associated with TEA did not provoke any alteration in the photochemical behavior of TRI. The results for the measured analytical parameters showed the success of the method. The standard curve was linear (r2 > 0.999) in the concentration range from 2 to 24 μg.mL -1. The method achieved good precision levels in the inter-day (relative standard deviation-RSD <3.4%) and reproducibility (RSD <3.8%) tests. The accuracy was about 80% and the pH changes introduced in the robustness study did not reveal any relevant interference at any of the studied concentrations. The experimental results demonstrate a simple, rapid and affordable UV-Vis spectrophotometric method that could be applied to the quantitation of TRI in this ternary complex.